Analysis of tetracycline antibiotics and their common impurities by high-performance liquid chromatography using a polymeric column

Yasin, Ahmed; Jefferies, T.M.

doi:10.1016/0731-7085(88)80103-1

Cited by 10 publications

(5 citation statements)

References 7 publications

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“…According to the literature, physicochemical methods are the most utilized in vivo and in vitro identification and quantification of DOX, within then, High Performance Liquid Chromatography (HPLC) has been considered the main one [3,4] and [12][13][14]. However, methods like capillary electrophoresis and spectrophotometry are present in those analyses as well and have the advantage of being more easily to handle [8] and [15][16][17].…”

Section: Equipmentmentioning

confidence: 99%

Short-Term Stability Study of Doxycycline Tablets by High Performance Liquid Chromatography, Spectrophotometry in the Ultraviolet Region and Turbidimetry

2018

JPCT

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Doxycycline, an antimicrobial, is available for free in the Brazilian Public System under medical prescription. Therefore, the population have easy access to it. Regarding quality control, doxycycline stability studies are important due to the epimerization reactions and the formation of degradation products under conditions that are not favourable to the drug leading to severe damages to the patient. So, the aim of this study was to develop a short-term stability study of doxycycline hyclate in intact tablet, pulverized tablets and in raw material. It utilized spectrophotometry in the Ultraviolet Region (UV), High Performance Liquid Chromatography (HPLC) and microbiologic method of turbidimetry. The combination of physicochemical and microbiological techniques is important in the sense that it is not enough only to identify and quantify the drug, but also to verify the activity. The short-term stability study proved that doxycycline hyclate in raw material, intact tablet and pulverized tablets was unstable under extreme conditions of heat and humidity 40ºC ± 2.0ºC and 75% ± 5.0%. The results were significantly different at time 0 and time 6. Raw material followed order zero degradation equations for spectrophotometry and HPLC and second order equation for turbidimetry. Intact tablet and pulverized tablets followed order zero equations for HPLC and second order equation for spectrophotometry and turbidimetry. There was a decrease in the antimicrobial activity and possible formation of degradation products that were detected at the final time of the study. The method can also be used in the test routine of pharmaceutical quality control for the efficacy and reliability of doxycycline tablets.

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Section: Equipmentmentioning

confidence: 99%

Short-Term Stability Study of Doxycycline Tablets by High Performance Liquid Chromatography, Spectrophotometry in the Ultraviolet Region and Turbidimetry

2018

JPCT

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“…The weak CL from TC is greatly increased by conversion to ATC. Dehydration of TC at C6 occurs in aqueous solutions at pH <2 [4] due to the presence of the hydroxyl group [23]. LC studies (Fig.…”

Section: Proposed Mechanismmentioning

confidence: 99%

“…These compounds may form during storage under adverse conditions of temperature and humidity [3]. Anhydro derivatives may also be found in out-of-date samples of TC [4]. These com-pounds are either inactive as antibiotics or toxic.…”

Section: Introductionmentioning

confidence: 99%

Determination of tetracycline and its major degradation products by chemiluminescence

Pena

Palilis

Lino

et al. 2000

Analytica Chimica Acta

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A fast and simple flow injection chemiluminometric method for the determination of trace amounts of tetracycline (TC) and its major degradation products epitetracycline (ETC), epianhydrotetracycline (EATC) and anhydrotetracycline (ATC) based upon the action of potassium hexacyanoferrate(III) in alkaline solution has been developed. The analytes can be determined with 10σ limits of quantification of 0.5 g for ETC, 2.0 g for TC, 0.01 g for EATC and 0.04 g for ATC. The sensitivity for TC is greatly improved by acidic degradation prior to the chemiluminescence (CL) measurement. The method developed allows measurement within the ranges of 0.040-2.0 g TC and ATC, 0.50-5.0 g ETC and 0.01-2.0 g EATC.

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“…On a timeline, if the mobile phases and columns of the previously used methods are compared (3,15), it is clear that the preparation time has improved, and methods are becoming more dynamic and easier to prepare. Regarding the running time of DOX, comparing the studied methods (3,16) shows that there was a decrease from more than 30 to 12 min.…”

Section: Introductionmentioning

confidence: 99%

Quantification of Doxycycline Hyclate in Tablets by HPLC–UV Method

Kogawa

Salgado

2012

Journal of Chromatographic Science

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An accurate, sensitive, precise and rapid gradient reversed-phase high-performance liquid chromatographic method was successfully developed and validated for the determination of doxycycline hyclate in bulk drug and tablets. The best separation was achieved on a 250 × 4.6 mm, 5.0 µm particle size CN Luna column with water + 0.1% TFA-acetonitrile + 0.1% TFA, 60:40 (v/v) as the mobile phase at a flow rate of 1.0 mL/min. Ultraviolet detection was performed at 360 nm at ambient column temperature (25°C). The method was linear over the concentration range of 50-100 µg/mL (r = 0.9999) with limits of detection and quantification of 2.83 and 8.59 µg/mL, respectively. The drug was subjected to oxidation, acid, base and neutral degradation, photolysis and heat as stress conditions. Degradation products were found interfering with the assay of doxycycline hyclate, therefore the method can be regarded as suitable. The method was applied for the determination of doxycycline hyclate in standard and pharmaceutical products, with excellent recoveries. The method can be used for the quality control of doxycycline hyclate.

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Analysis of tetracycline antibiotics and their common impurities by high-performance liquid chromatography using a polymeric column

Cited by 10 publications

References 7 publications

Short-Term Stability Study of Doxycycline Tablets by High Performance Liquid Chromatography, Spectrophotometry in the Ultraviolet Region and Turbidimetry

Short-Term Stability Study of Doxycycline Tablets by High Performance Liquid Chromatography, Spectrophotometry in the Ultraviolet Region and Turbidimetry

Determination of tetracycline and its major degradation products by chemiluminescence

Quantification of Doxycycline Hyclate in Tablets by HPLC–UV Method

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